CN115011976A - Lead-indium bimetallic catalyst and preparation method and application thereof - Google Patents
Lead-indium bimetallic catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a lead-indium bimetallic catalyst and a preparation method and application thereof, and is characterized in that the catalyst adopts lead indium metals with different proportions to form a powder nano material with a general formula of Pbx-Iny-X, wherein:xthe molar ratio of the lead metal is shown as,x=0.001~1；ythe mole ratio of the indium metal is shown as,y= 0.001-4; x is the calcining temperature, and X = 500-700 ℃. The catalyst is used as a cathode in an H-type electrolytic cell, an Ag/AgCl electrode, a platinum electrode and the cathode (catalyst) are respectively used as a three-electrode system of a reference electrode, a counter electrode and a working electrode, and a sulfuric acid aqueous solution is used as an electrolyte to carry out the selective electrocatalytic reduction of levulinic acid into valeric acid. Compared with the prior art, the method has the advantages of simple process, nano-scale particle size of the provided catalyst, good stability, and electrocatalytic reduction by levulinic acid to obtainThe selectivity and the catalytic activity of the valeric acid are higher.
Description
Technical Field
The invention relates to the technical field of metal catalysts, in particular to a lead-indium bimetallic catalyst, a preparation method thereof and application thereof in electrochemical reduction of levulinic acid into pentanoic acid.
Background
Excessive consumption of fossil fuels not only causes energy exhaustion, but also causes many environmental problems, and people have to search for clean energy which can be continuously developed. Among clean energy sources such as solar energy and wind energy, biomass can be used as the only sustainable carbon source, can be used for extracting liquid fuels, chemicals and polymer materials for traditional petroleum production, and attracts people's extensive attention. The lignocellulose biomass is more attractive to people, is cheap, clean and easily available, is not edible, and cannot cause competition to the food industry when being used in large quantities. In the process of chemical conversion and utilization of biomass, small molecular compounds, namely biomass platform molecules, can be derived, and can produce various high-value-added chemicals through various conversion modes. Levulinic acid produced from lignocellulosic biomass has attracted a great deal of attention from scientists as one of the biomass platform molecules.
Among various chemicals derived from levulinic acid, a "valeric acid biofuel" shows satisfactory performance when mixed with existing fuels, and valeric acid, which is an intermediate of the biofuel, can also be used for producing lubricants, perfumes, animal feeds, pharmaceuticals, etc., and thus, direct conversion of levulinic acid into valeric acid by a one-pot method has led scientists to extensive research. Noble metal or zeolite-type supports are frequently used as catalysts in thermodynamic oxidation or reduction, but deactivation of the catalysts by coking or metal leaching often occurs. In this respect, electrocatalytic reduction of levulinic acid into pentanoic acid using renewable electricity is more advantageous.
Since the 2012 use of electrochemical methods by Nilges et al, and the direct electrocatalytic reduction of levulinic acid to pentanoic acid from levulinic acid using lead metal as a cathode catalyst, many efforts to reduce levulinic acid from lead metal as an electrocatalyst have been extensively studied. The lead metal has higher selectivity for electrocatalytic reduction of levulinic acid due to higher hydrogen evolution overpotential, and can effectively inhibit hydrogen evolution reaction. Meanwhile, the selectivity for the generation of valeric acid is higher at a higher pH value and a lower potential. But simultaneously has certain problems, lead electrodes are easy to corrode under strong acid condition, so that the pollution of products is caused, and the separation is difficult; on the other hand, although lead metal is a non-noble metal, it is a harmful substance, which limits the research progress thereof.
Disclosure of Invention
The invention aims to provide a lead-indium bimetallic catalyst and a preparation method and application thereof aiming at the defects of the prior art, wherein lead metal is taken as an electrocatalyst, and another indium metal is added to form a powder material with a general formula of Pbx-Iny-X, Pbx-Iny-X is taken as a catalyst, a three-electrode system is adopted in an H-type electrolytic cell, an Ag/AgCl electrode, a platinum electrode and a cathode (catalyst) are respectively taken as a reference electrode, a counter electrode and a working electrode, and 0.5M H is adopted 2 SO 4 The aqueous solution is used as electrolyte, the selective hydrogenation of levulinic acid into valeric acid is efficiently electrocatalytic, the selectivity and Faraday efficiency are high, and the catalyst has certain stability and wide application prospect.
The purpose of the invention is realized as follows: a lead-indium bimetallic catalyst is characterized in that the molar ratio of the catalyst is 1: 4-1: 0.5 of lead-indium bimetal has the general formula of Pbx-Iny-X, wherein:xthe molar ratio of lead metal is 0.001-1;ythe molar ratio of indium metal is 0-4; x is the calcining temperature of 500-700 ℃.
A preparation method of a lead-indium bimetallic catalyst is characterized in that the lead-indium bimetallic catalyst adopts oleylamine surfactant as an additive, and is calcined in air by a hydrothermal method to synthesize the catalyst with a general formula as follows: the nano composite material of Pbx-Iny-X is prepared by the following steps:
a, step a: general formula (Pb), (OAc) 2 ·3H 2 O and In (NO) 3 ) 3 ·XH 2 O and deionized water 1 mmol: 0.5-4 mmol: mixing 20-60 mL of the mixture into solution A for later use;
b, step (b): mixing surfactant oleylamine and ethanol according to the ratio of 2-5: stirring and mixing the mixture into a solution B at a volume ratio of 10-25 for later use;
b, step (b): dropwise adding the prepared solution A into the solution B, stirring for 8-12 hours at normal temperature, reacting the formed precursor solution for 10-18 hours at the temperature of 100-200 ℃, naturally cooling to room temperature after the reaction is finished, centrifugally separating the reaction solution, washing the obtained product for several times by using a mixed solution of ethanol, ethanol and n-hexane in sequence, and drying for 8-24 hours at the temperature of 60-80 ℃ to obtain the compound with the general formula of Pbx-InyThe powder of (a) is a lead-indium bimetal composite material;
c, step (c): calcining the prepared lead-indium bimetal composite material in the air at the temperature of 500-700 ℃ at the speed of 2-5 ℃/min for 2-5 h to prepare the compound material with the general formula of Pbx-Iny-X, and-a lead-indium bimetallic catalyst.
The application of the lead-indium bimetallic catalyst prepared by the preparation method of the lead-indium bimetallic catalyst in the electro-catalytic reduction of valeric acid by levulinic acid is characterized in that the lead-indium bimetallic catalyst with the general formula of Pbx-Iny-X is used as a cathode in an H-type electrolytic cell, an Ag/AgCl electrode, a platinum electrode and the cathode (catalyst) are respectively used as a three-electrode system of a reference electrode, a counter electrode and a working electrode, and H is used 2 SO 4 The water solution is used as electrolyte to carry out the synthesis reaction of the selective electrocatalytic reduction of the levulinic acid into the valeric acid, the H-shaped electrolytic cell adopts a Nafion117 proton exchange membrane, the working voltage of the electrolytic cell is-1.2 to-1.6 VvsAg/AgCl, the anolyte of the H-shaped electrolytic cell is 0.1 to 0.5M levulinic acid solution and 0.4 to 0.8M H 2 SO 4 The solution is 0.4-0.8M H of catholyte 2 SO 4 And (3) solution. The Nafion117 film is a proton exchange film, and the working voltage of the electrolytic cell is controlled to be-1.2 to-1.6 VvsAg/AgCl; the electrocatalytic reaction time was 2 hours.
Compared with the prior art, the invention has the following remarkable technical effects and advantages:
1) prepared by a hydrothermal method and has the general formula of Pbx-InyThe powder catalyst has extremely high product selectivity, is easy to operate and relatively stable, can effectively improve the product selectivity under the condition of low potential, provides a new way for converting levulinic acid into biomass micromolecules with high added values, and has wide application prospect.
2) The use of bimetallic catalysts can, on the one hand, co-regulate the performance of the catalysts by means of a concerted effect, and on the other hand, can reduce the use of precious and harmful metals. Therefore, a new catalyst is needed to be developed, which can utilize the coordination effect between different metals to comprehensively utilize the advantages of the two, and a suitable bimetallic composite electrocatalyst is developed for the selective hydrogenation of levulinic acid to prepare pentanoic acid through electrocatalysis.
Drawings
FIG. 1 is a transmission electron microscope image of the product prepared in example 4;
FIG. 2 is an X-ray diffraction image of the product prepared in example 4;
FIG. 3 is a graph showing the activity of electro-catalyzing levulinic acid to pentanoic acid in examples 1-6;
FIG. 4 is a graph of the activity of electrocatalytic levulinic acid production of pentanoic acid of examples 4, 7 and 8.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
1) Preparing a precursor solution: adding 0.667 mmol Pb (OAc) 2 ·3H 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form a solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethanol, stirring and mixing to form a solution B, slowly dropwise adding the prepared solution A into the solution B, and stirring at normal temperature for 12 hours to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products with a mixed solution of ethanol, ethanol and n-hexane for a plurality of times in sequence, and drying in a drying oven at 70 ℃ under a temperature of a pedicle for 12 hours. Then, the powder product is the Pb-600 lead metal catalyst after being calcined in the air for 3 hours at the temperature of 600 ℃ and the speed of 2 ℃/min.
Example 2
1) Preparing a precursor solution: adding 0.667 mmol Pb (OAc) 2 ·3H 2 O and 0.334 mmol In (NO) 3 ) 3 ·XH 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form a solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethanol, stirring and mixing to form a solution B, slowly dropwise adding the prepared solution A into the solution B, and stirring at normal temperature for 10 hours to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products for a plurality of times by using mixed liquid of ethanol, ethanol and n-hexane in sequence, and drying in a drying oven at 70 ℃ for 10 hours. Then, calcining the mixture in air at a temperature of 600 ℃ and a speed of 2 ℃/min for 2 hours to obtain a powdery product Pb 2 -In 1 -600 lead-indium bimetallic catalyst.
Example 3
1) Preparing a precursor solution: adding 0.667 mmol Pb (OAc) 2 ·3H 2 O and 0.667 mmol In (NO) 3 ) 3 ·XH 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form a solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethanol, stirring and mixing to form a solution B, slowly dropwise adding the prepared solution A into the solution B, and stirring at normal temperature for 12 hours to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products for a plurality of times by using mixed liquid of ethanol, ethanol and n-hexane in sequence, and drying in a drying oven at 70 ℃ for 18 hours. Then, calcining the mixture in air at a temperature of 600 ℃ and a speed of 2 ℃/min for 5 hours to obtain a powdery product Pb 1 -In 1 -600 lead-indium bimetallic catalyst.
Example 4
1) Preparing a precursor solution: adding 0.667 mmol Pb (OAc) 2 ·3H 2 O and 1.334 mmol In (NO) 3 ) 3 ·XH 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethyl alcohol, and stirring and mixing to form solution BAnd slowly dripping the prepared solution A into the solution B, and stirring for 10 hours at normal temperature to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products for a plurality of times by using mixed liquid of ethanol, ethanol and n-hexane in sequence, and drying in a drying oven at 70 ℃ for 24 hours. Then, calcining the mixture in air at a temperature of 600 ℃ and a speed of 2 ℃/min for 3 hours to obtain a powdery product Pb 1 -In 2 -600 lead-indium bimetallic catalyst.
Example 5
1) Preparing a precursor solution: adding 0.667 mmol Pb (OAc) 2 ·3H 2 O and 2.668 mmol In (NO) 3 ) 3 ·XH 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form a solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethanol, stirring and mixing to form a solution B, slowly dropwise adding the prepared solution A into the solution B, and stirring at normal temperature for 12 hours to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products for a plurality of times by using mixed liquid of ethanol, ethanol and n-hexane in sequence, and drying in a drying oven at 70 ℃ for 20 hours. Then, calcining the mixture in air at a temperature of 600 ℃ and a speed of 2 ℃/min for 3 hours to obtain a powdery product Pb 1 -In 4 600 lead-indium bimetallic catalyst.
Example 6
1) Preparing a precursor solution: 1.334 mmol of In (NO) 3 ) 3 ·XH 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form a solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethanol, stirring and mixing to form a solution B, slowly dropwise adding the prepared solution A into the solution B, and stirring at normal temperature for 12 hours to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products for a plurality of times by using mixed liquid of ethanol, ethanol and n-hexane in sequence, and drying in a drying oven at 70 ℃ for 20 hours. Then, the powder product is the In-600 indium metal catalyst after being calcined In the air for 3 hours at the temperature of 600 ℃ and the speed of 2 ℃/min.
Example 7
1) Preparing a precursor solution: adding 0.667 mmol Pb (OAc) 2 ·3H 2 O and 1.334 mmol of In (NO) 3 ) 3 ·XH 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form a solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethanol, stirring and mixing to form a solution B, slowly dropwise adding the prepared solution A into the solution B, and stirring at normal temperature for 12 hours to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products for a plurality of times by using mixed liquid of ethanol, ethanol and n-hexane in sequence, and drying in a drying oven at 70 ℃ for 20 hours. Then, calcining the mixture in air at a temperature of 500 ℃ and a speed of 2 ℃/min for 3 hours to obtain a powdery product Pb 1 -In 2 -500 lead-indium bimetallic catalyst.
Example 8
1) Preparing a precursor solution: adding 0.667 mmol Pb (OAc) 2 ·3H 2 O and 1.334 mmol In (NO) 3 ) 3 ·XH 2 Dissolving O in 40 mL of deionized water, mixing and stirring to form a solution A, adding 4 mL of oleylamine solution into 20 mL of absolute ethanol, stirring and mixing to form a solution B, slowly dropwise adding the prepared solution A into the solution B, and stirring for 10 hours at normal temperature to obtain a precursor solution.
2) Transferring the prepared precursor solution into a hydrothermal kettle, reacting at 180 ℃ for 12 hours, naturally cooling to room temperature after reaction, centrifugally separating reaction liquid, washing obtained products with mixed liquid of ethanol, ethanol and n-hexane for a plurality of times, and drying at 70 DEG COven dried for 18 hours. Then, calcining the mixture in air at a speed of 2 ℃/min for 3 hours at a temperature of 600 ℃, and obtaining a powdery product Pb 1 -In 2 -700 lead-indium bimetallic catalyst.
The electrochemical reaction of levulinic acid reduction to pentanoic acid was carried out in an H-cell using any of the catalysts prepared in examples 1-8 as a cathode and a platinum mesh as an anode, and the anolyte was a 0.2M levulinic acid solution and 0.5M H 2 SO 4 Solution, catholyte 0.5M H 2 SO 4 The solution, Nafion117 film is proton exchange film, the electrolytic cell working voltage is controlled at-1.2 to-1.6 VvsAg/AgCl.
Referring to FIG. 1, Pb prepared in example 4 1 -In 2 TEM image of 600 catalyst material, from which it can be seen that the morphology of the composite lead-indium catalyst is uniform nano-particles, and the particle size is about 10 nm.
Referring to FIG. 2, Pb prepared in example 4 1 -In 2 -an XRD pattern of 600 catalyst materials,
it can be clearly observed that 2 O 3 And diffraction peaks of PbO confirm that PbO and In are contained In the composite Pd-In material 2 O 3 And coexisting. The diffraction peak of the composite material is broadened due to the reduction of the particle size of the formed catalyst after the lead-indium metal is mixed with each other.
Referring to FIG. 3, the working electrode was loaded with the nanocomposites prepared in examples 1-6, respectively, in 0.2M levulinic acid solution and 0.5M H 2 SO 4 The faradaic efficiency of the electrolytic production of pentanoic acid under-1.5 VvsAg/AgCl potential conditions was neutralized in solution. It can be seen that the catalyst has higher selectivity and catalytic activity for electrocatalytic levulinic acid hydrogenation. The mutual doping of the lead and indium metals has a synergistic effect and better catalytic activity than any single metal.
Referring to FIG. 4, the working electrode was loaded with the nanocomposites prepared in examples 4, 7, and 8, respectively, in 0.2M levulinic acid solution and 0.5M H 2 SO 4 The faradaic efficiency of the electrolytic production of pentanoic acid under-1.5 VvsAg/AgCl potential conditions was neutralized in solution. It can be seen that different calcination temperature pairsThe catalytic activity of the catalyst has certain influence, but the obtained nano composite materials have higher selectivity and Faraday efficiency on electrocatalytic reduction of levulinic acid into pentanoic acid through hydrogenation.
The invention has been described in further detail in order to avoid limiting the scope of the invention, and it is intended that all such equivalent embodiments be included within the scope of the following claims.
Claims (4)
1. A lead-indium bimetallic catalyst is characterized in that the molar composition general formula of the lead-indium bimetallic catalyst is as follows: pbx-Iny-X, wherein:xis the molar ratio of the lead metal, and the lead metal,x=0.001~1；ythe mole ratio of the indium metal is shown as,y= 0.001-4; x is the calcining temperature, and X = 500-700 ℃.
2. The preparation method of the lead-indium bimetallic catalyst of claim 1, characterized in that the lead-indium bimetallic catalyst adopts oleylamine surfactant as additive, and is calcined in air by a hydrothermal method to synthesize the catalyst with the general formula: the nano composite material of Pbx-Iny-X is prepared by the following steps:
a, step a: general formula (Pb), (OAc) 2 ·3H 2 O and In (NO) 3 ) 3 ·XH 2 O and deionized water 1 mmol: 0.5-4 mmol: mixing 20-60 mL of the mixture into solution A for later use;
b, step (b): mixing surfactant oleylamine and ethanol according to the ratio of 2-5: stirring and mixing the mixture into a solution B at a volume ratio of 10-25 for later use;
b, step (b): the solution A prepared above was mixed according to the following ratio 1: 0.6-1: dropwise adding the mixed solution into the solution B in a volume ratio of 0.4, stirring for 8-12 hours at normal temperature, reacting the formed precursor solution for 10-18 hours at the temperature of 100-200 ℃, naturally cooling to room temperature after the reaction is finished, and centrifugally separating the reaction solution to obtain a powdery product, namely the lead-indium bimetal composite material;
c, step (c): washing the obtained product with a mixed solution of ethanol, ethanol and n-hexane for several times in sequence, drying at the temperature of 60-80 ℃ for 8-24 h, calcining at the temperature of 500-700 ℃ for 2-5 h at the heating rate of 2-5 ℃/min, and preparing the general formulaIs Pbx-Iny-X nanocomposite lead-indium bimetallic catalyst.
3. The application of the lead-indium bimetallic catalyst prepared by the preparation method of the lead-indium bimetallic catalyst according to claim 2 in the electro-catalytic reduction of valeric acid by levulinic acid is characterized in that the lead-indium bimetallic catalyst is used as a cathode in an H-type electrolytic cell, and is subjected to a synthesis reaction of selective electro-catalytic reduction of levulinic acid into valeric acid with a three-electrode system consisting of a working electrode, a reference electrode and a counter electrode, wherein an Ag/AgCl electrode and a platinum electrode, and an anolyte of the H-type electrolytic cell is 0.1-0.5M levulinic acid solution and 0.4-0.8M H 2 SO 4 The solution is 0.4-0.8M H of catholyte 2 SO 4 And (3) solution.
4. The application of the lead-indium bimetallic catalyst prepared by the preparation method of the lead-indium bimetallic catalyst according to claim 2 in the electro-catalytic reduction of valeric acid by levulinic acid is characterized in that a Nafion117 proton exchange membrane is adopted in the H-type electrolytic cell, the working voltage is-1.2 to-1.6 VvsAg/AgCl, and the electro-catalytic reaction time is 2 hours.
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